CN111624218A - Non-destructive method for analyzing distribution characteristics of chemical elements on surface of three-dimensional fossil and cultural relic - Google Patents
Non-destructive method for analyzing distribution characteristics of chemical elements on surface of three-dimensional fossil and cultural relic Download PDFInfo
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Abstract
The invention relates to a non-destructive three-dimensional fossil and cultural relic surface chemical element distribution characteristic analysis method, which comprises the following steps: fixing a sample, detecting the position and surface characteristics of the sample and generating a solid geometric model of the sample; selecting a space range or a surface area of a model to be analyzed of a sample to be detected according to the solid geometric model of the sample; setting measurement parameters, a running track and a detection point of detection equipment and a light spot diameter of X-ray focusing which can reach micron level; according to the element characteristic spectral line of each analysis point on the set running track, the content of the element required to be known is given, and the surface space distribution characteristics of the element content of the measured surface, the area to be measured or the complete sample surface of the sample are obtained according to the element content of each point on the measured surface or the whole solid sample surface. The analysis method can realize the aim of carrying out non-destructive automatic analysis on the surface elements of the fossil and the cultural relic (such as the head bone of the ape, the vase or the three-dimensional cultural relic).
Description
Technical Field
The invention relates to the technical field of nondestructive automatic chemical component analysis of fossil and cultural relic, in particular to a nondestructive analysis method for the distribution characteristics of chemical elements on the surfaces of three-dimensional fossil and cultural relic.
Background
The analysis of the chemical composition and distribution characteristics of cultural relics and fossil surfaces is of great importance for the understanding of the sources, characteristics, structures and histories of these materials (Lijunfeng, dawn Xia, 2018), as well as for the restoration and repair of cultural relics (Likunfei et al 2010; Litao, 2010), biological evolution and ancient earth environment research (Liyuxing, 2000; Litao et al 2008; Dumont et al, 2009), and researchers can even explore the artistic thoughts and creation processes of the authors according to the sequence of use of pigments at different positions and layers of oil paintings (De Meyer et al, 2019).
The existing analysis equipment usually requires that a sample to be detected is ground into solid powder and tabletted, and the destructive treatment mode cannot meet the detection requirement of preserving intact samples such as cultural relics or fossil stones. Conventional non-destructive analysis of samples involves processing the sample to be tested into a flat surface and placing it in a sample chamber dedicated to the analytical equipment (jion et al, 2005; von rosy clouds et al, 2007; zhangongheng et al, 2019), which is difficult to process large samples such as dinosaur fossils due to the space constraints of the analytical equipment and the sample chamber. Samples that require the determination of three-dimensional surface elemental composition characteristics, such as a cultural crock or simian skull (Buddhachat et al, 2016; Nganvongpanit et al, 2017), are more difficult to process. The existing non-destructive analysis can only carry out small-area scanning or single-point analysis (such as an electron microscope and energy spectrum analysis thereof) on the uniform surface of a tiny sample, while a high-energy particle fluorescence energy spectrum device can only carry out nondestructive element analysis on a plane sample or a spherical sample with a large area, but is not suitable for large cultural relics and large fossil (such as dinosaur skeletal fossil with the weight of several tons) with irregular surfaces, and the development of scientific research and the exploration of early civilization and the like are seriously hindered.
Microbeam X-ray fluorescence scanning is an emerging technology (tourmaline et al, 2011; Church et al, 2016; Manukyan et al, 2016; Hampai et al, 2017) developed in recent years, which can scan and detect planar fossil or small ceramic wafers in a small sample chamber. The analysis area is greatly improved compared with the scanning energy spectrum analysis of an electron microscope, but the requirement of detecting a large-area sample still cannot be met due to the detection setting of a tiny area. The conventional common equipment can only detect with fixed resolution and cannot adjust the size of an X-ray spot, so that the conventional common equipment cannot meet the detection requirement beyond the preset resolution of an instrument, namely, the conventional common equipment needs to consume several months or years when micron-scale scanning is performed on large-scale fossil or cultural relics.
At present, Bruker Nano company in Germany develops a three-axis motion XRF analyzer (Alfeld et al, 2013; Vandivere et al, 2019), which can analyze the surface characteristics of chemical elements of a planar sample (Bergmann et al, 2012), but the chemical element composition characteristics of an irregular sample cannot be analyzed or have a great error, and the huge analysis error caused by the diffuse reflection of the surface of a rough sample cannot be processed (Jiong et al, 2005; Beckhoff et al, 2007).
The references mentioned above are specifically as follows (in alphabetical order by author):
Alfeld,M.,Pedroso,J.V.,van Eikema Hommes,M.,Van der Snickt,G.,Tauber,G.,Blaas,J.,Haschke,M.,Erler,K.,Dik,J.and Janssens,K.,2013.A mobileinstrument for in situ scanning macro-XRF investigation of historicalpaintings.Journal of Analytical Atomic Spectrometry,28(5),pp.760-767.
Beckhoff,B.,Kanngieβer,B.,Langhoff,N.,Wedell,R.and Wolff,H.eds.,2007.Handbook of practical X-ray fluorescence analysis.Springer Science&Business Media.
Bergmann,U.,Manning,P.L.and Wogelius,R.A.,2012.Chemical mapping ofpaleontological and archeological artifacts with synchrotron X-rays.AnnualReview of Analytical Chemistry,5,pp.361-389.
Buddhachat K,Klinhom S,Siengdee P,et al.Elemental Analysis of Bone,Teeth,Horn and Antler in Different Animal Species Using Non-Invasive HandheldX-Ray Fluorescence[J].PLOS ONE,2016,11(5).
Church,J.,Meirer,F.,Keune,K.,Mehta,A.and Mass,J.,2016.Analyticalimaging studies of the migration of degraded orpiment,realgar,and emeraldgreen pigments in historic paintings and related conservation issues.
De Meyer,S.,Vanmeert,F.,Vertongen,R.,van Loon,A.,Gonzalez,V.,van derSnickt,G.,Vandivere,A.and Janssens,K.,2019.Imaging secondary reactionproducts at the surface of Vermeer’s Girl with the Pearl Earring by means ofmacroscopic X-ray powder diffraction scanning.Heritage Science,7(1),p.67.
Dumont,M.,Zoeger,N.,Streli,C.,Wobrauschek,P.,Falkenberg,G.,Sander,P.M.and Pyzalla,A.R.,2009.Synchrotron XRF analyses of element distribution infossilized sauropod dinosaur bones.Powder Diffraction,24(2),pp.130-134.
Hampai,D.,Liedl,A.,Cappuccio,G.,Capitolo,E.,Iannarelli,M.,Massussi,M.,Tucci,S.,Sardella,R.,Sciancalepore,A.,Polese,C.and Dabagov,S.B.,2017.2D-3DμXRF elemental mapping of archeological samples.Nuclear Instruments andMethods in Physics Research Section B:Beam Interactions with Materials andAtoms,402,pp.274-277.
Manukyan,K.V.,Guerin,B.J.,Stech,E.J.,Aprahamian,A.,Wiescher,M.,Gura,D.T.and Schultz,Z.D.,2016.Multiscale X-ray fluorescence mapping complementedby Raman spectroscopy for pigment analysis of a 15th century Bretonmanuscript.Analytical Methods,8(42),pp.7696-7701.
Nganvongpanit,K.,Buddhachat,K.,Piboon,P.,Euppayo,T.andMahakkanukrauh,P.,2017.Variation in elemental composition of human teeth andits application for feasible species identification.Forensic scienceinternational,271,pp.33-42.pp.39-45.
Speakman,R.J.and Shackley,M.S.,2013.Siloscience and portable XRF inarchaeology:a response to Frahm.Journal of Archaeological Science,40(2),pp.1435-1443.
Vandivere,A.,van Loon,A.,Callewaert,T.,Haswell,R.,Gaibor,A.N.P.,vanKeulen,H.,Leonhardt,E.and Dik,J.,2019.Fading into the background:the darkspace surrounding Vermeer’s Girl with a Pearl Earring.Heritage Science,7(1),p.69.
tunlin, plum blossom field, Jinyou Stone, Yanchangsheng, Wangshi, & Li Shuwu, et al (2011). method for analyzing ancient porcelain high-lead glaze by microbeam X-ray fluorescence nondestructive analysis and application research.
Von rosy clouds, li guild, fan loyal, panyan mountain, fanui, 2007. X-ray fluorescence spectrometer and its application study in geology mineral rock geochemistry bulletin, (z1), pp.592-594.
Jieon, Dougeny, Zhuorijun, Rogli.
Lijunfeng, wangxiao, 2018 research on nondestructive identification of mineral pigments of mural cultural relics by visible spectroscopy, spectroscopy and spectral analysis, 38(1), pp.200-204.
Plum, 2010. nondestructive chemical analysis of ancient paper relics in china (scientific discservation, doctor thesis of university of the chinese academy of sciences and scientific archaeology).
Li billow, Qin Ying, Luo Wu gan, Teng Jian, Zhao Peng, Liu bin, Wang Xiao Ni, 2008. ancient bronze ware corrosion products Raman and infrared spectroscopy analysis nonferrous metals, 60(2), pp.146-152.
Prunus salicina, 2000. neutron activation analysis of dinosaur embryos study, proceedings of the institute of Wuhan chemical industry, 22(4),
bear cherry phenanthrene, Gongyuwu Wu Jing Wei, Xijundin, Wu Jing Wei, 2010. Shangling lake Yueku celadon body glaze EDXRF analysis of chemical composition cultural relics protection and archaeology science, (4), pp.28-34.
Zhang Wenchui, Cao Ji Xiang Zhang Shuang, 2019. X-ray fluorescence spectrometry for determining lead, tellurium and bismuth in free-cutting stainless steel, metallurgy analysis, 39(3), pp.38-43.
Disclosure of Invention
In order to solve the prior technical problems, the invention provides a non-destructive method for analyzing the distribution characteristics of chemical elements on the surfaces of three-dimensional fossil and cultural relics,
the system is realized by an operation interface module, a software and hardware communication module, a detection device movement control module, a detection device, a multi-channel data analysis module, a data qualitative and quantitative analysis module, a data image processing module, a sample surface geometric characteristic acquisition and analysis module and a sample surface diffuse reflection correction module, wherein the detection device comprises an X-ray light pipe and controller, an X-ray lens and controller, an X-ray fluorescence energy spectrum receiver and controller;
the operation interface module is respectively connected with the detection equipment movement control module, the X-ray light pipe and controller, the X-ray lens and controller, and the X-ray fluorescence energy spectrum receiver and controller through the software and hardware communication module; the operation interface module is also connected with a multi-channel data analysis module, a data qualitative and quantitative analysis module, a data image processing module, a sample surface geometric characteristic acquisition and analysis module and a sample surface diffuse reflection correction module; the operation interface module is used for configuring control information and processing data, and directly receiving analysis data of the multi-channel data analysis module, or is connected with other modules through a software and hardware communication module and controls each module;
the X-ray light pipe and the controller comprise an X-ray emitter and a current and voltage control unit of the X-ray light pipe, and the unit can determine the intensity and wavelength emitted by the X-ray emitter according to the characteristics of the element measured by the analysis sample; the X-ray lens and the controller focus the X-ray and adjust the distance between the lens and the sample to form a light spot on the surface of the sample; the X-ray fluorescence energy spectrum receiver and the controller are used for collecting X-ray data and sending the X-ray data to the operation interface module through the multi-channel data analysis module; the multi-channel data analysis module is used for uploading all the acquired data in the detection process to the operation interface module, and the sample surface diffuse reflection correction module scans and analyzes all the side surfaces and irregular surface types of the sample and corrects the detection result;
the analysis method comprises the following steps:
s1, fixing a fossil or cultural relic sample, detecting the position and the surface characteristic of the sample through a data image processing module and/or a sample surface geometric characteristic acquisition and analysis module, and generating a sample solid geometric model through an operation interface module;
s2, selecting a space range or a surface area of a model to be analyzed by the sample to be detected according to the solid geometric model of the sample by the operation interface module;
s3, setting measurement parameters, the running track and the detection site of the detection equipment and the spot diameter of X-ray focusing reaching micron level through manual selection or operation of the interface module, and sending the measurement parameters to the detection equipment movement control module, the X-ray light tube and controller, the X-ray lens and controller, the X-ray fluorescence energy spectrum receiver and controller;
and S4, giving the content of the element which needs to be known according to the element characteristic spectral line of each analysis point on the set running track, and obtaining the surface space distribution characteristics of the element content of the measured surface, the area to be measured or the complete sample surface of the sample according to the element content of each point on the measured surface or the whole solid sample surface.
Further, fixing the sample on a sample table in S1, detecting the position, the stereo image and the shape feature of the sample through a data image processing module and/or a sample surface geometric feature acquisition and analysis module, and transmitting the generated stereo geometric model to an operation interface module; in S2, the spatial range or the surface area of the model to be analyzed of the sample to be tested is selected manually or automatically by operating the interface module.
Furthermore, the sample surface geometric feature acquisition and analysis module comprises a laser radar or a laser range finder, the laser radar or the laser range finder determines the position information of each position on the surface of the sample according to the distance between the laser and the surface of the sample, and transmits the received data to the operation interface module for data processing, so that the three-dimensional structure spatial feature model of the sample is obtained.
Furthermore, in S3, the measurement parameters set by the operation interface module or manually include parameters of the detection device movement control module, the X-ray tube and controller, the X-ray lens and controller, and the X-ray fluorescence energy spectrum receiver and controller, and the measurement parameters are transmitted to the corresponding module through the software and hardware communication module, and the X-ray tube and controller, the X-ray lens and controller, and the X-ray fluorescence energy spectrum receiver and controller are respectively arranged at the front end of the detection device movement control module and controlled by the detection device movement control module; the detection equipment movement control module controls the size of a focusing light spot of the X-ray lens, the X-ray fluorescence energy spectrum receiver and the controller to move to the surface normal direction of the sample to be detected, and the distances between the X-ray fluorescence energy spectrum receiver and the controller and the sample to be detected are adjusted and the X-ray fluorescence energy spectrum receiver and the controller move in different directions in space.
Further, when the measurement parameters are determined in S3, the sample surface diffuse reflection correction module is used to correct the diffuse reflection deviation of the X fluorescence measurement, the sample surface diffuse reflection correction module irradiates the sample surface with a non-destructive laser beam, the attenuation characteristic parameters of diffuse reflection and angular scattering are obtained from the reflection characteristics of the light beam on the sample surface, the reflection characteristics are determined by the reflection intensity received by the sensor, so as to correct the surface characteristic interference in the X fluorescence measurement, and when the X fluorescence receiver cannot reach the normal direction of the measured surface, the diffuse reflection correction module corrects the data reception in the non-normal direction.
Further, the X-ray tube and the controller in S3 include an X-ray emitter and an X-ray tube current-voltage control unit, the X-ray tube current-voltage control unit controls the X-ray emitter according to the physical characteristics of the sample element to be analyzed, and the current-voltage control unit adjusts the intensity and wavelength of the X-ray emitted by the X-ray emitter and controls the movement of the X-ray; and the data acquired by the X fluorescence energy spectrum receiver is transmitted to the multi-channel data analysis module, and the multi-channel data analysis module transmits the acquired data to the operation interface module.
Further, in S4, a standard curve of the content of the element to be known is determined by the data qualitative and quantitative analysis module according to the fluorescence intensity of the standard sample element and the concentration of the corresponding element, and the analysis result is output to the operation interface module by the software and hardware communication module.
Furthermore, the working state of the system is recorded through a photographic imaging module in the measuring process, the photographic imaging module is arranged at the front end of the detection equipment movement control module and comprises a camera, the camera records the running state of the display equipment and the image characteristics of the measured position in real time and displays the image in real time, and the photographic imaging module fuses the collected surface image to the geometric model of the three-dimensional fossil and cultural relic.
Furthermore, the data transmission mode in the measurement process comprises a serial port bus 485, a USB bus, a PCI bus, an Ethernet or a CAN bus, the software and hardware communication module transmits the data acquired by the sensor to the operation interface module, and the operation interface module transmits the execution command to the actuator and the data acquisition unit.
Furthermore, the light spot of the X-ray is adjusted according to the measurement precision requirement, and when micron-sized high-resolution detection is required, the X-ray light spot is adjusted to be micron-sized through the X-ray lens, the controller and the detection equipment movement control module.
The invention obtains the subsidies of the strategic leading science and technology special item (XDB26000000) of the Chinese academy of sciences, the National Science Foundation Committee (NSFC) and the assistance of the modern ancient biology and stratigraphic national key laboratory (Nanjing geological ancient biology institute).
The invention has the beneficial effects that: the analysis method can carry out three-dimensional modeling on the shape of the object on the basis of not damaging the structure of the object to be detected, sets measurement parameters and a measurement range on the basis of the three-dimensional modeling, obtains the chemical element composition of the surface of the solid material and the distribution characteristics of the accurate content of the chemical element composition of the surface of the solid material by scanning and analyzing all the side surfaces and the irregular surfaces of the object, and realizes the aim of carrying out non-destructive automatic analysis on the surface elements of the fossil and the cultural relic (such as the skull of an ape, a vase or the three-dimensional cultural relic).
Drawings
The following further explains embodiments of the present invention with reference to the drawings.
FIG. 1 is a schematic diagram of the method for analyzing the distribution characteristics of chemical elements on the surface of nondestructive three-dimensional fossil and cultural relic;
FIG. 2 is a system diagram of the nondestructive analysis method for the distribution characteristics of chemical elements on the surfaces of three-dimensional fossil and cultural relic according to the present invention;
FIG. 3 is a schematic view of the detection result obtained by the analysis method of the present invention 1;
FIG. 4 is a schematic diagram of the detection results obtained by the analysis method of the present invention 2.
Detailed Description
As shown in fig. 1 and fig. 2, this embodiment discloses a method for analyzing distribution characteristics of chemical elements on the surface of nondestructive three-dimensional fossil and cultural relic, wherein the device and method are as follows:
the device mainly comprises an operation interface module 1, a software and hardware communication module 2, a photographic imaging module 3, a detection device movement control module 4, an X-ray light pipe and controller 5, an X-ray lens and controller 6, an X-ray fluorescence energy spectrum receiver and controller 7, a multi-channel data analysis module 8, a data qualitative and quantitative analysis module 9, a data image processing module 10, a sample surface geometric characteristic acquisition and analysis module 11 and a sample surface diffuse reflection correction module 12, wherein the X-ray light pipe and controller 5, the X-ray lens and controller 6 and the X-ray fluorescence energy spectrum receiver and controller 7 are detection devices.
The operation interface module 1 is respectively connected with the photographic imaging module 3, the detection equipment movement control module 4, the X-ray light pipe and controller 5, the X-ray lens and controller 6 and the X-ray fluorescence spectrum receiver and controller 7 through the software and hardware communication module 2; the operation interface module 1 is also connected with a multi-channel data analysis module 8, a data qualitative and quantitative analysis module 9, a data image processing module 10, a sample surface geometric characteristic acquisition and analysis module 11 and a sample surface diffuse reflection correction module 12. The operation interface module 1 mainly performs configuration and data processing of related control information, and directly receives analysis data of the multi-channel data analysis module 8, or is connected with other modules through the software and hardware communication module 2 and controls each module.
The software and hardware communication module 2 is used for data communication, the transmission mode in the measurement process comprises a serial port bus 485, a USB bus, a PCI bus, an Ethernet or a CAN bus, the software and hardware communication module 2 transmits data collected by sensors (including an X-ray fluorescence energy spectrum detector, an anti-collision detector, a distance sensor and the like) to the operation interface module 1, and the operation interface module 1 transmits execution commands to actuators (such as a motion controller, an X-ray tube controller and the like) and data collectors (such as a laser radar, a position and distance collector, various actuators and sensors and the like).
The multi-channel data analysis module 8 is used for transmitting all the acquired data in the detection process to the operation interface module 1, so that a user can check the comprehensive analysis result.
The analysis method comprises the following steps:
s1, fixing a fossil or cultural relic sample, detecting the position and the surface characteristic of the sample through a data image processing module and/or a sample surface geometric characteristic acquisition and analysis module, and generating a sample solid geometric model through an operation interface module;
s2, selecting a space range or a surface area of a model to be analyzed by the sample to be detected according to the solid geometric model of the sample by the operation interface module;
s3, setting measurement parameters, the running track and the detection site of the detection equipment and the spot diameter of X-ray focusing reaching micron level through manual selection or operation of the interface module, and sending the measurement parameters to the detection equipment movement control module, the X-ray light tube and controller, the X-ray lens and controller, the X-ray fluorescence energy spectrum receiver and controller;
and S4, giving the content of the element which needs to be known according to the element characteristic spectral line of each analysis point on the set running track, and obtaining the surface space distribution characteristics of the element content of the measured surface, the area to be measured or the complete sample surface of the sample according to the element content of each point on the measured surface or the whole solid sample surface. The detection of the position and surface features of the sample and the generation of the solid geometric model of the sample in S1 are performed by the data image processing module 10 and/or the sample surface geometric feature acquisition and analysis module 11. The image and graph processing module acquires a three-dimensional image and shape characteristics of a solid material sample, and the acquired characteristics are analyzed and then used for constructing external parameters in sample detection, so that a region to be detected and a precision range are determined, and a reasonable scanning approach and a safe motion track are ensured. In this embodiment, the sample surface geometric feature acquisition and analysis module 11 includes a laser radar or a laser range finder, and the laser radar or the laser range finder determines distances from various positions on the surface of the sample by sending laser to the solid sample, so as to obtain position information of various points on the surface of the sample. The laser radar or the laser range finder transmits the measured data to the operation interface module 1 for processing.
The operation interface module 1 generates a three-dimensional spatial feature model of the solid sample according to the collected three-dimensional structural data of the sample, and in S2, the operation interface module 1 determines the spatial range to be measured of the sample surface or the surface area of the model according to the model.
In S3, the interface module 1 is manually selected or operated to set measurement parameters according to the determined space range or surface area to be measured, and the measurement parameters mainly aim at each actuator, such as the detection device movement control module 4, the X-ray light pipe and controller 5, the X-ray lens and controller 6, and the X-ray fluorescence spectrum receiver and controller 7.
In this embodiment, the detection device movement control module 4 is a space and angle adjustable movement controller, and the X-ray light pipe and controller 5, the X-ray lens and controller 6, and the X-ray fluorescence spectrum receiver and controller 7 are disposed at the front end thereof.
The X-ray tube and controller 5 includes an X-ray emitter and current and voltage control unit of the X-ray tube that can determine the intensity and wavelength emitted by the X-ray emitter based on the characteristics of the element being measured by the analysis sample. The X-ray lens and controller 6 is an X-ray lens and distance controller for focusing X-rays and adjusting the distance between the lens and the sample to form a suitable light spot on the surface of the sample. The X-ray fluorescence spectrum receiver and controller 7 is used for collecting X-ray data and sending the X-ray data to the multi-channel data analysis module 8.
The detection device movement control module 4 is used for moving the focusing light spot of the X-ray lens and the X-ray fluorescence energy spectrum detector to the surface normal direction of the measured position of the solid material sample, and adjusting the distance between the focusing light spot and the measured position, so that the reliable composition and content characteristics of the surface elements of the sample are obtained. The module also has an anti-collision function for the sample. The module can be additionally provided with an independent motion control unit of the X-ray lens so as to further adjust the size of an X-ray spot and adapt to the detection resolution required by various samples.
The detection device movement control module 4 controls the distance between the X-ray light pipe and the X-ray emitter of the controller 5 and the sample and the X-ray lens and the X-ray spot of the controller 6. The control instruction is sent from the operation interface module 1 through the software and hardware communication module 2, and comprises the switch, the current and the voltage of the X-ray tube, and the X-ray intensity and the wavelength emitted by the X-ray tube are controlled. The X fluorescence spectrum receiver transmits the collected data to the multi-channel data analysis module 8 for processing. The detection equipment movement control module 4 controls the distance between the X-ray lens and the sample, so that the size of the X-ray spot can be controlled, and the diameter of the spot required by analysis can reach a micron level.
The detection device mobile control module 4 of this embodiment can adjust the X-ray light spot through two methods, and in the actual detection and analysis process, can select independent or joint control X-ray light spot size according to the detection requirements of different resolutions (such as millimeter level or micron level), can adapt to the detection requirements of different types of samples under different environments, and save the time of scanning analysis.
In S3, in order to improve the detection accuracy, the sample surface diffuse reflection correction module 12 scans and analyzes all the sides and irregular surfaces of the sample, and corrects the detection result. The correction value for each position of the sample is related to the x-ray tube direction and the sensor position and direction. A determined sample surface characteristic (including surface gloss, distance and angle) and the relative position and angular difference between the X-ray tube and the sensor will have a determined correction factor that is obtained using laser detection and used to correct XRF (X-ray fluorescence analyzer) analysis data. In this embodiment, the sample surface diffuse reflection correction module 12 irradiates a sample surface with a non-destructive laser beam, and obtains attenuation characteristic parameters of diffuse reflection and angular scattering through a reflection characteristic of the light beam on the sample surface (the reflection characteristic can be measured by receiving reflection intensity with a sensor), so as to correct surface characteristic interference in X-ray fluorescence measurement. Through the correction of the sample surface diffuse reflection correction module 12, the error detected by the X fluorescence spectrum receiver and the controller 7 is reduced, and the specific process is as follows: the X fluorescence energy spectrum receiver and the controller 7 inputs the detection data to the operation interface module 1 through the multi-channel data analysis module 8, and the operation interface module 1 processes the data of the X fluorescence energy spectrum receiver and the controller 7 according to the geometric model and the surface diffuse reflection correction module 12.
In S4, the set element characteristic spectral line of each analysis point on the running trajectory is realized by the data qualitative and quantitative analysis module 9, the data qualitative and quantitative analysis module 9 is configured to create a standard curve with different element contents, and determine the standard curve according to the fluorescence intensity of the standard sample element and the concentration of the corresponding element. In the detection process, standard samples can be inserted at fixed intervals (time/sample number), and the standard samples can also be inserted at any time according to the detection requirement so as to correct detection value drift possibly occurring in the detection process. During analysis, a sample area needing to be analyzed, such as a certain surface, a certain area or a complete surface, is selected, elements needing to be known or researched are selected, and the corresponding element content surface spatial distribution characteristics can be generated according to the detected element content of each point on the surface of the solid sample, so that the nondestructive analysis of cultural relic and fossil surface elements is realized.
Preferably, the camera imaging module 3 is further provided for displaying the operation state of the device and the image characteristics of the measured position in real time during the measurement, and displaying the real-time images of the operation of each device to the operator. On one hand, the monitoring and recording effect can be achieved, the working state of the actuator can be displayed in real time, and an operator can observe the record conveniently; on the other hand, the method can realize the measurement and recording of samples with different specifications in different scenes, and for the element analysis in non-laboratory scenes, a user can also visually observe the motion process of each device, thereby enlarging the application scene range of the method. The camera imaging module 3 can be used to fuse the collected surface image to the geometric model of the three-dimensional fossil and cultural relic (such as color, texture, etc., which can obtain the real image of the cultural relic or the fossil).
The analysis method disclosed in this embodiment uses small and micro components, such as a micro X-ray tube, so that it is possible to install these high-integration light components in the detection device mobile control module. The front-end components can move in different directions under the drive of the detection equipment movement control module, so that the scanning of chemical element composition of each surface to be detected of the three-dimensional sample is realized. Meanwhile, a three-dimensional model and a spatial position of the sample are obtained through a sample surface geometric analysis module, and after a motion track is accurately calculated, the sample is scanned and measured through the combination of an X-ray light pipe and controller 5, an X-ray fluorescence spectrum receiver and a controller 7. The required resolution ratio of the size control of the X-ray irradiation light spot can be changed by changing the position of the X-ray tube and the sample or the distance between the X-ray lens and the sample so as to meet the detection resolution ratio requirements of different users on different samples, the content or the composition of chemical elements of the point is obtained by combining a diffuse reflection correction module, and the element composition distribution characteristic of the surface of the measured sample is given according to the space geometric position of each point.
Fig. 3 is a schematic diagram of an application result of the embodiment, which is a schematic diagram of detecting and obtaining an element distribution of stellera fin fossil. The left side of the sample mace fossil is the content distribution of the Fe element in the sample mace fossil, and the right side of the sample mace fossil is the content distribution of the Fe element in the sample mace fossil. It can be seen that, by using the method of the embodiment, the shape of the obtained element content distribution diagram is approximately the same as that of the stellera fin fish fossil, and the element content distribution conforms to the actual situation.
Fig. 4 is a schematic diagram of another application result of this embodiment, which is a schematic diagram of detecting and obtaining element distribution of Guizhou dragon fossil. The left side of the Guizhou dragon fossil is a sample to be detected, the right side of the Guizhou dragon fossil is a Ca element content distribution diagram, the higher the content of the element in the result diagram is, the darker the color displayed in the diagram is, and the darker the color of the body part of the Guizhou dragon fossil in fig. 4 shows that the content of the Ca element in the body part of the Guizhou dragon fossil is high, so that the practical situation of the Ca element content distribution in the Guizhou dragon fossil is met.
In the previous description, numerous specific details were set forth in order to provide a thorough understanding of the present invention. The foregoing description is only a preferred embodiment of the invention, which can be embodied in many different forms than described herein, and therefore the invention is not limited to the specific embodiments disclosed above. And that those skilled in the art may, using the methods and techniques disclosed above, make numerous possible variations and modifications to the disclosed embodiments, or modify equivalents thereof, without departing from the scope of the claimed embodiments. Any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the scope of the technical solution of the present invention.
Claims (10)
1. A non-destructive three-dimensional fossil and cultural relic surface chemical element distribution characteristic analysis method is characterized by comprising the following steps:
the system is realized by an operation interface module, a software and hardware communication module, a detection device movement control module, a detection device, a multi-channel data analysis module, a data qualitative and quantitative analysis module, a data image processing module, a sample surface geometric characteristic acquisition and analysis module and a sample surface diffuse reflection correction module, wherein the detection device comprises an X-ray light pipe and controller, an X-ray lens and controller, an X-ray fluorescence energy spectrum receiver and controller;
the operation interface module is respectively connected with the detection equipment movement control module, the X-ray light pipe and controller, the X-ray lens and controller, and the X-ray fluorescence energy spectrum receiver and controller through the software and hardware communication module; the operation interface module is also connected with a multi-channel data analysis module, a data qualitative and quantitative analysis module, a data image processing module, a sample surface geometric characteristic acquisition and analysis module and a sample surface diffuse reflection correction module; the operation interface module is used for configuring control information and processing data, and directly receiving analysis data of the multi-channel data analysis module, or is connected with other modules through a software and hardware communication module and controls each module;
the X-ray light pipe and the controller comprise an X-ray emitter and a current and voltage control unit of the X-ray light pipe, and the unit can determine the intensity and wavelength emitted by the X-ray emitter according to the characteristics of the element measured by the analysis sample; the X-ray lens and the controller focus the X-ray and adjust the distance between the lens and the sample to form a light spot on the surface of the sample; the X-ray fluorescence energy spectrum receiver and the controller are used for collecting X-ray data and sending the X-ray data to the operation interface module through the multi-channel data analysis module; the multi-channel data analysis module is used for uploading all the acquired data in the detection process to the operation interface module, and the sample surface diffuse reflection correction module scans and analyzes all the side surfaces and irregular surface types of the sample and corrects the detection result;
the analysis method comprises the following steps:
s1, fixing a fossil or cultural relic sample, detecting the position and the surface characteristic of the sample through a data image processing module and/or a sample surface geometric characteristic acquisition and analysis module, and generating a sample solid geometric model through an operation interface module;
s2, selecting a space range or a surface area of a model to be analyzed by the sample to be detected according to the solid geometric model of the sample by the operation interface module;
s3, setting measurement parameters, the running track and the detection site of the detection equipment and the spot diameter of X-ray focusing reaching micron level through manual selection or operation of the interface module, and sending the measurement parameters to the detection equipment movement control module, the X-ray light tube and controller, the X-ray lens and controller, the X-ray fluorescence energy spectrum receiver and controller;
and S4, giving the content of the element which needs to be known according to the element characteristic spectral line of each analysis point on the set running track, and obtaining the surface space distribution characteristics of the element content of the measured surface, the area to be measured or the complete sample surface of the sample according to the element content of each point on the measured surface or the whole solid sample surface.
2. The method according to claim 1, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: s1, fixing the sample on a sample table, detecting the position, the three-dimensional image and the shape characteristic of the sample through a data image processing module and/or a sample surface geometric characteristic acquisition and analysis module, and transmitting the generated three-dimensional geometric model to an operation interface module; in S2, the spatial range or the surface area of the model to be analyzed of the sample to be tested is selected manually or automatically by operating the interface module.
3. The method according to claim 2, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: the sample surface geometric feature acquisition and analysis module comprises a laser radar or a laser range finder, the laser radar or the laser range finder determines the position information of each position on the surface of the sample according to the distance between laser and the surface of the sample, and transmits the received data to the operation interface module for data processing, so that the three-dimensional structure spatial feature model of the sample is obtained.
4. The method according to claim 1, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: the measurement parameters set through the operation interface module or manually in the S3 include parameters of the detection device movement control module, the X-ray light pipe and controller, the X-ray lens and controller, the X-ray fluorescence energy spectrum receiver and controller, and the measurement parameters are transmitted to the corresponding module through the software and hardware communication module, the X-ray light pipe and controller, the X-ray lens and controller, the X-ray fluorescence energy spectrum receiver and controller are respectively arranged at the front end of the detection device movement control module and controlled by the detection device movement control module; the detection equipment movement control module controls the size of a focusing light spot of the X-ray lens, the X-ray fluorescence energy spectrum receiver and the controller to move to the surface normal direction of the sample to be detected, and the distances between the X-ray fluorescence energy spectrum receiver and the controller and the sample to be detected are adjusted and the X-ray fluorescence energy spectrum receiver and the controller move in different directions in space.
5. The method according to claim 4, wherein the analysis method for the distribution characteristics of the chemical elements on the surfaces of the non-destructive three-dimensional fossil and cultural relic comprises: when the measurement parameters are determined in the S3, the sample surface diffuse reflection correction module is used for correcting the diffuse reflection deviation of the X fluorescence measurement, the sample surface diffuse reflection correction module irradiates a sample surface with a non-destructive laser beam, the attenuation characteristic parameters of diffuse reflection and angle scattering are obtained through the reflection characteristics of the light beam on the sample surface, the reflection characteristics are determined by receiving the reflection intensity through the sensor, so that the surface characteristic interference in the X fluorescence measurement is corrected, and when the X fluorescence receiver cannot reach the normal direction of the measured surface, the diffuse reflection correction module corrects the data reception in the illegal line direction.
6. The method according to claim 4, wherein the analysis method for the distribution characteristics of the chemical elements on the surfaces of the non-destructive three-dimensional fossil and cultural relic comprises: the X-ray tube and the controller in the S3 comprise an X-ray emitter and an X-ray tube current and voltage control unit, wherein the X-ray tube current and voltage control unit controls the X-ray emitter according to the physical characteristics of the sample element to be analyzed, and adjusts the intensity and wavelength of X-rays emitted by the X-ray emitter and controls the movement of the X-rays; and the data acquired by the X fluorescence energy spectrum receiver is transmitted to the multi-channel data analysis module, and the multi-channel data analysis module transmits the acquired data to the operation interface module.
7. The method according to claim 1, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: and in S4, determining a content standard curve of the element to be known according to the fluorescence intensity of the standard sample element and the concentration of the corresponding element by a data qualitative and quantitative analysis module, and outputting the analysis result to an operation interface module by a software and hardware communication module.
8. The method according to claim 1, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: the working state of the system is recorded through the camera imaging module in the measuring process, the camera imaging module is arranged at the front end of the detection equipment movement control module and comprises a camera, the camera records the running state of the display equipment and the image characteristics of the measured position in real time and displays the image in real time, and the camera imaging module fuses the collected surface image to the geometric model of the three-dimensional fossil and cultural relic.
9. The method according to claim 1, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: the data transmission mode in the measurement process comprises a serial port bus 485, a USB bus, a PCI bus, an Ethernet or a CAN bus, the software and hardware communication module transmits data collected by the sensor to the operation interface module, and the operation interface module transmits an execution command to the actuator and the data collector.
10. The method according to claim 1, wherein the analysis method for the distribution characteristics of chemical elements on the surface of the non-destructive three-dimensional fossil and cultural relic comprises: and adjusting the X-ray light spot according to the measurement precision requirement, and when micron-sized high-resolution detection is required, reducing the X-ray light spot to the micron-sized through an X-ray lens, a controller and a detection equipment movement control module.
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